Stable waterproofing composition



Patented Feb. 4, 1941 UNITED STATES PATENT OFFICE 2,230,656 STABLE WATERPROOFING COMPOSITION Adolph Scholler, Philadelphia, Pa.; The Pennsylvania Company for Insurances on Lives and Granting Annuities and Fred C. Scholler, executors for Adolph Scholler, deceased, assignors to Scholler Brothers, Inc., Philadelphia, Pa., a corporation of Pennsylvania No Drawing. ApplicationNovember 20, 1937,

Serial No. 175,589

16 Claims. (01. 134-15) My invention relates to compositions for. delusstable concentrated emulsion containing an inorganic inert delustrant and a waterproofing agent for textiles, and to dilute the concentrated emulsion as desired to produce a one-bath delustering and water repelling treatment.

A further purpose is to produce a concentrated stable dispersion of an inorganic inert delustrant and a wax, such as parafiin, in the presence 'of aluminum sulphate or "an equivalent, and to .dilute the concentrated emulsion to treat textile fibers and fabrics, especially silk or rayon in a single bath. I

A further purpose is to subject textile fibers A further purpose is to avoid any reaction between aluminum'sulphate and a stabilizing agent and to render ,the dispersion stable over a wide temperature range by employing a starch of substantially uniform viscosity over'the climatic temperature range to stabilize the dispersion of a delustering, waterproofing and finishing composition. Y J

A further purpose is to treat. textile fibers and fabrics with a dispersion including a wax, an inorganic inert'delustrant, aluminum sulphate or the equivalent, soap or the equivalent, gelatine or the equivalent, and starch, thereby delusteriiig. waterproofing and finishlng 'the fiber. or fabric. Further, purposes appear in the specification and in'the claims.

The invention relates both to'the methods employed and to the composltionsp'roduced.

For the sake of simplicity, the invention will be explained as it is applied to fabrics such as silk or rayon, particularly ladies stockings.

In the prior practice, where a delustrant and a waterproofing agent were applied to the textile fibers or fabrics in one bath, the bath was made up by separate additions of the delustrant and luster,

the waterproofing agent to the diluted bath. Usually the fiber. or fabric was treated with,the

delustrant bath before the waterproofingagent was added, or vice versa. This prior practice has been unnecessarily time consumin Dartic'u- .5 larly where a relatively small amount of fiber or fabric was undergoing treatment.

, As a result of investigation, it has been found possible, in accordance .wlththe present invention, to make up a thoroughly stable concentrated emulsion which includes both the delustrant and the waterproofing agent, and todllute thisconcentrat- 1 ed emulsion at one operation to form a single bath which applies both the delustrant and the waterproofing agent to thefiber or fabric. The dilution is usually made by adding water until the dilute bath is 50 to 400 times the volume of the concentrated emulsion. In any casethe dilute bath will have more than ten times the volume of the concentrated emulsion.

A particular application of the present inventionis to the delustering, waterproofing and finishing of ladies silk or rayon stockings which have lost, by repeated washing, the delustering,

waterproofing and finish applied by themanufacturer. It is not "possible for the housewife to treat the stockings by the methods used at the time of manufacture, because of the complexity,

the need-of equipment and the special conditions required. But it is possible for the housewife by the present invention to restore the deluster, the waterproofing, and thefinish in a single bath without complex equipment. The concentrated emulsion of the invention will keep indefinitely in any climate, and satisfactorily treat silk, rayon, wool, cotton, linen, etc., fibers and fabrics, either at the time of manufacture or to restore the properties lost by wear and washing.

, Similarly. the'invention may be used by the textile manufacturer.

Y The treating composition is applied to thetextile material in the form of a dispersion in water.

As sold, the dispersionwill be quite concentrated,

but for use it may be diluted to say fifty to four hundred volumes or more by adding water. By

among its disperse phases an inorganic inert delustrant, and a wax which assists in waterproofing and finishing. Aluminum sulphate or the equivalent is also present to cooperate with other ingredients and assist in waterproofing and finlshing.

Soap is very desirably included in the composition, since it is itself an emulsifying agent, and it will combine with the aluminum salt or the equivalent, producing an aluminum or equivalent salt of the fatty acid which also functions as an emulsifying and waterproofing agent and imparts a finish'to the fabric.

In order to prevent coagulation or flocculation ofthe colloid on long standing, to maintain the dips'ersion stable at the high dilutions employed during use and to prevent precipitation with marked change in temperature, it. is important.v to add a stabilizing agent in addition to the emulsifying agent which assists in forming the dispersion and has the property of keeping the wax and the delustrant in stable dispersion. The presence of, the j aluminum sulphate or the equivalent makes it much more difiicult to obtain a satisfactory stabilizer. Gums of vari- I ous sorts such as gum trag'acanth, which might otherwise be used, react with the aluminum sulphate or the equivalent and lose'their efliciency asstabilizers. Emulsifying agents such as glue and gelatine liquefy and lose body at elevated temperatures, and therefore they will not withstand the wide'variations in temperature ofiered 'by climatic conditions in various parts of theinhabited world.

After extensive experimentation, the present an inventor has discovered that certain starches are not aifected by aluminum sulphate or the equivalent, and also have substantially uniform viscosity over the temperature. ranges encoun-- tered in various climates. As the starches'in- The present inventor has discovered, further more, that starches of substantially uniform viscosity over the climatic temperature range have desirable finishing properties, impartingbody and sealing to textile fibers and fabrics.

The most satisfactory starch known to appli cant for the present purpose is tapioca, since it does not fiocculate in the presence of aluminum sulphate or the equivalent and does not substantially change its viscosity 'over the climatic It also possesses finishing temperature ranges. properties.

The delustrant use should be inorganic and A mat to the other ingredients. Organic delustrants (such as zinc or aluminum stearate, oleate or palmitatel can only be dispersed in very 'small concentrations to produce stable suspensions. As the waxisuch asv paraflin) tends to increase the luster, the small quantitie of organic delustrants which could be placed in stable dispersion are'inefiective to overcome the lus- .tering influence of the wax and impart substantial delusteringproperties to the composition.

v oxide, bismuthoxide, barium sulphide or barium carbonateare not inert, but react with some v other ingredient (for example tapioca) and m form an insoluble substance which spots the While the invention may be embodied in a wide variety'of diiferent compositions, one example of. theingredients and one example of 1 the manner of compounding and the desirable Certainl inorganic delustrants such as izinc proportions will be given, recognizing that other compositions and other methods of compound-' ing may be devised by those skilled in the art.

As a delustrant any suitable -finely' divided insoluble inorganic metallic salt, inert to the 6 other ingredients, may be emplo ed. It is preferred to'use titanium oxide oxide), barium sulphate or a mixture of the two such as Tita'nox B. Less satisfactory but commercial results may be obtained with barium oxide, lead oxide, zirl0 conium oxide or lead sulphate.

The delustrant is ground to a suitably fine state of subdivision before incorporating in the treating composition of the invention, and then is dispersed in water-in suitable manner, using 15 an emulsifier (machine) for example.

The quantity of delustrant must be more than sufiicient to overcome any lustering effect of the wax, where wax is present.

A dispersion of wax is also used in the com- 20 .position'. The wax is preferably paraflln; although any suitable wax such as chlorinated naphthalene, petroleum Jelly or petrolatum, Japan wax, montan wax, eandelilla wax, ozokerite or carnauba ,wax might be used. The wax 1' is dispersed in a suitable manner, as for example by melting it, incorporating a protective colloid,

and passing the water mixture containing the molten 'wax through an emulsifier.

' Aluminum sulphate imparts considerable acid- 30 ity; and it is usually desirable to reduce the acidity somewhat by an alkali. Instead of aluminum sulphate, another soluble salt of a polyvalent (having a valence of two, three or more) metal, possessing the property of imparting 35 water-repellency and finish to the textile, may be used. Of course, if the solution of the salt ishighly colored or stains the fiber or fabric, it would be objectionable. Among the equivalents which might be used,. instead of aluminum Q sulphate, alum, aluminum acetate, aluminum formate, basic aluminum formate, zinc sulphate, zinc acetate, zinc formate, etc., may be suggested. L

A very useful ingredient of the treating composition is soap or the equivalent. Among the soaps which may be used, sodium or potassium ,stearate, oleate' or palmitate is particularly recommended. As an equivalent of'soap, a sulso phonated oil, a fatty alcohol, a fatty alcohol sulphonate, etc., may be employed...

As a protective colloid it is preferred to use gelatine, although glue may: be employed instead k of gelatine. A preservative is desirably em-'65 .ployed along with the gelatine or glue: for example, formaldehyde, benzoic acid or sodium tribenzoate. One of these preservatives is suitably .used with the'starch, also. The point at which the preservative is added is not critical.

According to the preferred method of compounding .and in the preferred proportions. to makeabout loo'pounds of a mixture used as an 7 intermediate in making the composition, the fol- M lowing ingredients are employed:

ished compositions In Liquid A, the soap solution (1' pound anhydrous soap in 20pounds of water) is made up separately from the gelatine solution (5.5 pounds gelatine in 23 pounds of water) and the soap and gelatine solutions are mixed preferably at about to F. (61 t0 76.5 fC,). Melted parafiin (20 pounds) is incorporated and the mixture is passedthrough'an emulsifier until it is thoroughly emulsified. A r Liquid B is made up separately by dissolving pounds), separately dissolving the soda ash (0.5 pound) in water (2, pounds) and mixing the soda ash' solution and the aluminum sulphate solution. The formaldehyde (0.2 pound) is then added to Liquid B, Liquids Aand B are mixed and the mixture is run through an emulsifier] The emulsified mixture of Liquids A and B is used in making up about 100 pounds of the fin- Pounds Emulsified mixture of Liquids A and B-.. 30.0 Tapioca 7.0 Water ....-.f:;. 50.0 Titanium oxide (dioxide) 5.0 Water I 5.0 Benzoic acid or formaldehyde 2.0

( Total ..-....99.0

The tapioca (7 pounds) is dissolved in hot water (50 pounds), the titanium oxide (5 pounds) is separately made into a paste 'with water (5 pounds) and the emulsified mixture of Liquids A and B, the starch solution, the titanium oxide' paste and the benzoic acid or formaldehyde are mixed together while hot and run through an emulsifier until thoroughly dispersed.

In the finished composition as sold (concentrated emulsion) and before dilution for .use, it has been found that the quantity of paraflln or the like should be from about 2 to 10%, preferably about 6%, thatof inorganic inert delustrant should be from about 1 to 8%, preferably about 5%,-that of aluminum sulphate or the equivalent should be from about 0.5% to 5%, preferably'about 2.5%, that of stabilizer should be from about 3 to 10%, preferably about 7%, that of soap or the equivalent should be from about 0.1 to 0.5 preferably about 0.3% and that of a protective colloid, (gelatine) should be from about 0.05 to 0.5%, preferably about 0.2%. N l It will of course be understood that the quantitles mentioned above may be varied, and, as

noted in the claims and elsewhere in the specification, some of the ingredients may be omitted. Other ingredients which do not harmfully affect the compositionmay be added. The above description of the actual composition as preferably made according to the invention is intended as a specific example merely, subject to variation by those skilled in the art.

The-product made in the above manner is a heavy paste, and may be kept indefinitely in a vessel such as a collapsible tube or jar, notwithstanding the normal climatic temperature changes of the Temperate Zone or the Tropics.

.Freezing will not harmthe composition.

- The starch. of. substantially constant viscosity ,over the climatic temperature changes stabilizes The parafiin assists inwaterproofing and hasflnishing properties, sealing the fiber or fabric and lubricating it. The gelatine, besides reacting with; aluminum to produce a waterproofing the aluminum sulphate (8 pounds) in water. (20

compound, also serves as a protective colloid. All of the ingredients serve to seal the individual strands, filaments or fibers.

In compounding the above composition, the formaldehyde may be added with the benzoic acid instead of at the time that Liquids A and B aremixed, if so desired, although if the mixture of Liquids A and B is not to be changed immediately into thefinished composition, the

presence of formaldehyde in the mixture of- Liquids A and B prevents decomposition. Either the formaldehyde or benzoic acid may be omitted if desired.

After the concentrated dispersion is made up as stated, it may be kept indefinitely in a container. Before use the concentrated dispersion will be diluted with water to at least ten volumes, and 1 preferably to fiftyor four hundred volumes or more. Where the composition is used to'deluster, waterproof and finish stockings, a small quantity, perhaps 3 or 5 cubic centimeters or less of the concentrated emulsion, diluted with water to fifty or four hundred volumes, will satisfactorily treat a pair of stockings, which are simply dipped several times or shaken in the dilute dispersion after they have been washed and rinsed and before they are hung up or boarded to dry.

Some advantages from the present invention may be obtained even though the wax be omitted or' even though-the delustrant be omitted, but the satisfaction obtained by the user is greatly in-: creased where both the wax and the delustrant are present, along with the aluminum sulphate or equivalent, the starch stabilizer, and desirably the soap or equivalent and the protective colloid.

In view of my invention, and disclosure variations'andmodifications to meet individual whim or particular need will doubtless become evident to others skilled in the art, to obtain all or part of the benefits of my invention without copying the methods and compositions described, and I,

therefore, claim all such in so far as they fall within the reasonable spirit and scope of my invention.

Having thus described my invention, what I Patent is:

claim as new and desire to secure by Letters a I s 70 1. A stable concentrated dispersion in water, 7 which on dilution with water serves as' a textile- 4 I -2,2a o,csa

than sufilcient to overcome any lustering effect 01' the wax, and tapioca.

.2. A stable concentrated dispersion in water, which on dilution with water serves as a textiletreating composition operating in a single bath, which comprises from 2% to of a wax, from 1% to 8% of an inorganic delustrant inert to the other ingredients, and from 3% to 10% of tap-.

ioca.

.10 3. A textile waterproofing composition com- --prising a stable concentrated dispersion of a wax in water, aluminum sulphate and tapioca.

4. A textile-treating composition containing a disperse phase, a soluble salt of a polyvalent .1 metal possessing the propertyoi' imparting water-repellency and finish to the textile, and tap- 5. A composition for delustering silk or rayon operating in a. single bath and comprising a stable concentrated dispersion in water of from 1% to 8%, or an inorganic delustrant inert to the other ingredients, from 0.5% to 5% of a soluble salt of a polyvalent metal possessing the property of imparting water-repellency and finish to the 25 textile, and from 3% to 10% of tapioca.

6. A composition fondelustering silk or rayon operating in a single bath and comprising a-stable concentrated dispersion in water of from 1% to 8% of an inorganic delustrant inert to the 30 other ingredients, from 0.5% to 5% of aluminum sulphate and from 3% to 10% of tapioca.

.-- 7. A delustrant composition for textiles operating in a single bath at dilutions of from 50 to 400 volumes and comprising an inorganic delustrant inert to other ingredients, dispersed in water, from 0.5% to 5% of a soluble Salt of a. polyvalent metal possessing the property of impart- I in'gwater-repellency and finish to the textil b soap and tapioca.

8. A delustrant composition for textiles operating in a single bath at dilutions of from 50 to 400 volumes and comprising from 1-% to 8% or an inorganic delustrant inert to the other ingradients, dispersed in water, 'i'rom 0.5% to 51% of aluminum sulphate, from 0.1%.to 0.5% of soap and tapioca.

9.A textile delustering, .waterproofing and finishing composition operating in 'a single bath 5; and comprising a stable concentrated dispersion in water of from 2% to 10% of a wax, from 1% to 8% of aninorganic delustrant inert to the other ingredients, from 0.5% to 5% or a soluble v salt of a polyvalent metal possessing the property .55 oi imparting 'water repellency and finish to the textile, from 0.1% to 5% or soap and from 3% to-10% of tapioca.

. 10. A textile .Idelusteringi waterproofing and lfinishing composition operating in a single bath 10%-dilutions of from 50 1:0,400 volumes and comprising a. stable concentrated dispersion in water of irom 2% to 10%/of a wax, irom 1%. to 8% of an inorganic delustrant inert to the other ingredients, from 0.5% to 5% of aluminum sulphate, from 0.1% to 5% of soap and from 3% to 10% of tapioca.

11. A textile deluster ing, waterproofing and finishing composition operating in a single bath at dilutions of from 50 to 400 volumes and comprising a dispersion in water of from 2% to 10% 'of a wax, from 1% to 8% of an inorganic" de-.

lustrant inert to the other ingredients, from 0.5% to 5% of a soluble salt of a polyvalent metal possessing the, property 'of imparting water-repellency and finish to the textile, from 0.05% to 0.5% of gelatine and from 3% to 10% of tapioca.

12. A textile delustering, waterproofing a'nd finishing composition operating in a singlebatli at dilutions of from 50 to 400 volumes and comprising a dispersion in water of from 2% to 10% of a wax, from 1% to 8% of an inorganic delustrant inert to the other ingredients, from 0.5% to 5% of aluminum sulphate, from 0.05% to 0.5% of gelatine and from 3% to 10% of tapioca.

13. A delustering, waterproofing and finishing composition for silk and rayon operating in a single bath at dilutions of from 5.0 to 400 volumes and comprising a dispersion in water of from 2% to 10% of a wax, from 1% to 8% of an inorganic delustrant inert to the other ingredients, from 0.5% to 5% of a soluble salt of a polyvalent metal possessing the property of imparting water-re pellency and finish to the textile, from 3% to 10% of tapioca, from 0.1% to 5% of soap and from 0.05% to 0.5% of gelatine.

l4. A'delustering, waterproofing and finishing composition for silk and rayon operating in a single bath-at dilutions of from 50to 400 volumes and' comprising a dispersion in water -of from polyvalent metal possessing the property of imparting water-repellency and finish to the textile,

soap and tapioca.

16. A textile delustering, waterproofing and;

finishing composition comprising a stable concentrated dispersion in. water of a wax, aninin quantity more than sufilcient to overcome any lustering effect of the wax, a soluble salt of a parting water-repellenc'y and finish to the textile, gelatine and tapioca.

ADOLPl-I SCHOLLER. 1

1 organic delustrant inert to the other ingredients,

.polyvalent metal possessing the property 01' im- 

